РАЗРАБОТКА КОМПЛЕКСА МАСС-СПЕКТРОМЕТРИЧЕСКИХ С ИНДУКТИВНО СВЯЗАННОЙ ПЛАЗМОЙ МЕТОДИК ОПРЕДЕЛЕНИЯ СОДЕРЖАНИЯ ИЗОТОПА ТЕХНЕЦИЙ-99 В УРАНОВЫХ МАТЕРИАЛАХ
Аннотация
Описан комплекс методик определения содержания изотопа технеций-99 (99Тс) в урановых материалах, основанный на методе масс-спектрометрии с индуктивно связанной плазмой. Приведены результаты исследования матричного влияния урана на аналитический сигнал 99Тс для двух моделей масс-спектрометров. Исследованы возможности метода для определения содержания 99Тс в различных вариантах: с предварительным отделением урана и прямого анализа. Разработанные масс-спектрометрические методики, основанные на экстракционно-хроматографическом разделении урана и 99Тс на смолах UTEVA и TEVA (Eichrom Technologies), отличаются низкими пределами обнаружения (0.0006-0.02 нг/г). Предлагаемые условия прямого масс-спектрометрического определения содержания 99Тс позволяют отказаться от «жестких» условий работы масс-спектрометров, требующих установления высокой мощности высокочастотного генератора (1600 Вт). Основными достоинствами разработанного комплекса являются значительное сокращение длительности и трудоемкости выполнения анализа по сравнению с радиометрическими методиками. Внедрение разработанных методик позволит усовершенствовать комплекс методик, используемых в системе контроля качества урановых материалов, действующих на предприятиях атомной отрасли.
Ключевые слова:масс-спектрометрия с индуктивно связанной плазмой, изотоп технеций-99, фториды урана, оксиды урана, экстракционно-хроматографическое разделениеПолный текст:
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ASTM International. Standards worldwide. Available at: http://www.astm.org (accessed 27 June 2013).
Tekhnicheskie usloviia 95.466-2007. Urana geksaftorid ot 1.0 % do 5.0 % obogashcheniia po izotopu urana-235 [Specification 95.466-2007. Uranium hexafluoride enriched from 1.0 % to 5.0 % 235U]. Moscow, VNIIHT, 2007. 22 р. (in Russian)
Tekhnicheskie usloviia 95.2523-2011. Urana geksaftorid syr'evoi sublimatnogo proizvodstva [Specification 95.2523-2011. Feeding uranium hexafluoride of sublimate manufacture]. Moscow, VNIIHT, 2011. 26 р. (in Russian).
Tekhnicheskie usloviia 95.2524-94 Urana geksaftorid syr'evoj razdelitel'nogo proizvodstva [Specification 95.2524-94. Feeding uranium hexafluoride of separate manufacture]. Moscow, VNIIHT, 1994. 15 р. (in Russian)
Murata M. Reprocessed uranium experience on conversion and enrichment in Japan // Proc. Technical Committee Meeting held in Vienna (Austria). August. 2007. 202 р.
Spitsyn V.I., Kuzina A.F. Tekhnetsii [Technetium]. Moscow, Nauka, 1981. 210 р. (in Russian).
Sapozhnikova N.V., Naumova Ju.A., Egorova O.N., Lumpov A.A., Babin V.A. [Determination of 99Tc in a water solution with using optical emission spectrometry with inductively coupled plasma Varian 725-ES]. Radiohimija [Radiochemistry], 2012, vol. 54, no 6, pp. 542-545 (in Russian).
Otraslevaia instruktsiia 001.471-2009. Tekhnetsii-99. Metodika radiometricheskogo opredeleniia v zakisi-okisi i geksaftoride [Standard 001.471-2009. Technetium-99. Standard test method for analysis of uranous uranic oxide and uranium hexafluoride by radiometry]. Novouralsk, UEIP, 2009. rsFR.31.2009.00456. 45 p. (in Russian)
Chu N. Y., Foldstein J. Radiochemical determination of technetium-99. Talanta, 1984, vol. 3, no. 10A, pp. 809-813.
Otraslevaia instruktsiia 001.575-2009. Tekhnetsii-99. Metodika mass-spektrometricheskogo s induktivno-sviazannoi plazmoi opredeleniia soderzhaniia v geksaftoride i zakisi-okisi urana [Standard 001.575-2009. Technetium-99. Standard test method for analysis of uranium hexafluoride and uranous uranic oxide by inductively coupled plasma mass-spectrometry]. Novouralsk, UEIP, 2009. rsFR.31.2009.00440. 38 p. (in Russian).
Saprygin A.V., Golik V.M., Kisel T.A., Trepachev S.A. [Direct (without radiochemical separation) determination of Tc-99 in uranium materials by ICP-MS]. Analitika i kontrol' [Analytics and control], 2005, vol. 9, no. 4, pp. 410-416 (in Russian).
Potter D. The Determination of Technetium in a Uranic Matrix Using ICP-MS // Agilent Technologies. Publication number 5965-5148EN, 2000, 5 p.
Monoshima N., Sayad N. Determination of Tc-99 in coastal seawater collected in Fukuoka . J. Radioanal. Nucl. Chem, 1995, vol. 197, no. 2, pp. 245-251.
Richter R.C., Koirtyohann S.R., Jurisson S.S. Determination of technetium-99 in aqueous solutions by inductively coupled plasma mass spectrometry: effects of chemical form and memory. J. Anal. At. Spectrom, 1997, vol. 12, no. 5, pp. 557-562. doi: 10.1039/A606483C .
Ihsannulah K. Significance and initial investigations for the separation of molybdenium from the anion exchange resin prior to technetium analysis by ICP-MS. J. Radioanal. Nucl. Chem, 1995, vol. 191, no. 1, pp. 67-73.
Medvedeva I.B., Kuznetsova N.A., Rovnyi S.I. Sorbtsiia. [Tc(VII) sorption by fibrous sorbents]. Atomnaia energiia [Nuclear energy], 2003, vol. 94, no 5, pp. 367-374 (in Russian).
Boulyga S.F., Testa C., Desideri D., Becker J.S. Optimization and application of ICP-MS and alpha-spectrometry for determination of isotopic ratios of depleted uranium and plutonium in samples collected in Kosovo. J. Anal. At. Spectrom, 2001, vol. 16, no. 11, pp. 1283-1289. doi: 10.1039/B103178N.
Monoshima N., Sayad M., Kakiuchi H., Maeda Y. Technetium-99 distribution in Pacific Ocean. Radiochimiya, 1977, vol. 39, no. 4, pp. 321-324.
Alvarado J. S., Erikson M. D. Determination of long-lived radioisotopes using electrothermal vaporization inductively coupled plasma. J. Anal. At. Spectrom, 1996, vol. 11, no. 10, pp. 923-928. doi: 10.1039/JA9961100923.
Beals D. M. Determination of technetium-99 in aqueous samples by isotope dilution inductively coupled plasma mass spectrometry. J. Radioanal. Nucl. Chem, 1996, vol. 204, no. 2, pp. 253-263.
Smith M. R., Wyse E. J. Radionuclide detection and analysis: a comparison of radiation counting and mass- spectrometric (ICP-MS) capabilities. Materials of the 38th ASMS conference on mass spectrometry and allied topics, 1990, vol. 1735, pp. 1439-1440.
Ihsanullah K. Methods for the separation of technetium from ruthenium for inductively coupled plasma mass spectrometry. Separation Science and Technology, 1994, vol. 29, no. 6, pp. 781-797.
Otraslevaia instruktsiia 001.542-2002. Tekhnetsii-99. Metodika mass-spektrometricheskogo s induktivno sviazannoi plazmoi opredeleniia v ZOU i GFU [Standard 001.542-2002. Technetium-99. Standard test method for analysis of uranium uranous uranic and oxide hexafluoride by inductively coupled plasma mass-spectrometry]. Novouralsk, UEIP, 2002, 45 p. (in Russian).
Uchida S., Tagami K. Separation of Tc-99 in soil and plant sample collected around the Chernobyl reactor using a Tc-selective chromatographic resin and determination of nuclide by ICP-MS. Appl. Rad. Isot, 2000, vol. 53, no. 1-2, pp. 69-73.
Tc-99 Faster than ever. Eichrom Ideas, 1998, vol. 5, no. 2, pp. 2.
Horwitz E. P., Chiarizia R., Dietz M. L., Diamond H. Separation and preconcentration of actinides from acidic media by extraction chromatography. Anal. Chim. Acta, 1993, vol. 281, no. 2, pp. 361-372.
Horwitz E.P., Dietz M.L., Chiarizia R., Diamond H., Maxwell III S.L., Nelson M.R. Separation and preconcentration of actinides by extraction chromatography using a supported liquid anion exchanger: Application to the characterization of high-level nuclear waste solutions. Anal. Chim. Acta, 1995, vol. 310, no. 1, pp. 63-78.
Horwitz E.P., Dietz M. L., Chiarizia R., Essling A. M., Graczyk D. Separation and preconcentration of uranium from acidic media by extraction chromatography. Anal. Chim. Acta, 1992, vol. 266, no. 1, pp. 25-37.
Golik V.M., Golik S.V., Prosviryakova A.V., Saprygin A.V., Trepachev S.A. [Usage of UTEVA resin for separation of uranium and impurities produced non-volatile and volatile fluorides in uranium hexafluoride]. Analitika i kontrol' [Analytics and control], 2011, vol. 15, no 2, pp. 174-181 (in Russian).
Golik V.M., Kisel T.A., Trepachev S.A. [Quantitative determination of impurities in uranium materials by mass spectrometry with inductively coupled plasma]. Mass-spektrometriia [Mass spectrometry], 2005, vol. 2, no 4, pp. 291-296 (in Russian).
Evans E.H., Caruso J.A. Optimization strategies for the reduction of non-spectroscopic interferences in inductively coupled plasma mass spectrometry. Spectrochimica Acta, 1992, vol. 47B, no. 8, pp. 1001-1012.
Mokhodoeva O.B., Miasoedova G.V., Zakharchenko E.A. [Solid-phase extractants for radionuclide preconcentration and separation. New possibilities]. Radiokhimiia [Radiochemistry], 2011, vol. 53, no. 1, pp. 34-41 (in Russian).
Evans Е.К, Giglio J.J. Interferences in inductively coupled plasma mass spectrometry. A review. J. Anal. At. Spectrom, 1993, vol. 8, no. 1, pp. 1-18. doi: 10.1039/JA9930800001.
Tan S. H., Horlick G. Matrix-effect observations in inductively coupled plasma mass spectrometry. J. Anal. At. Spectrom, 1987, vol. 2, no. 8, pp. 745-763. doi: 10.1039/JA9870200745 .
Agatemor C., Beauchemin D. Matrix effects in inductively coupled plasma mass spectrometry: A review. Analytica Chim. Acta, 2011, vol. 706, no. 1, pp. 66-83.
Wang J., Shen W.-L., Sheppard B. S., Evans E. H., Caruso J. A., Fricke F. L. Effect of ion-lens tuning and flow injection on non-spectroscopic matrix interferences in inductively coupled plasma mass spectrometry. J. Anal. At. Spectrom, 1990, vol. 5, no. 6, pp. 445-449. doi: 10.1039/JA9900500445.
Wang J., Evans E. H., Caruso J. A. Minimization of non-spectroscopic matrix interferences for the determination of trace elements in fusion samples by flow injection inductively coupled plasma mass spectrometry. J. Anal. At. Spectrom,1991, vol. 6, no. 8, pp. 605-608. doi: 10.1039/JA9910600605.
Evans E. H., Caruso J. A. Optimization strategies for the reduction of non-spectroscopic interferences in inductively coupled plasma mass spectrometry. Spectrochim. Acta. Part B, 1992, vol. 47, no. 8, pp. 1001-1010.
Karandashev V. K., Leikin A. Iu., Zhernokleeva K. V. [Reduction of matrix effects in ICP–MS by optimizing settings of ion optics]. Zhurnal analiticheskoi khimii [Journal of analytical chemistry], 2014, vol. 69, no. 1. pp. 1-9 (in Russian, unpublished).
Blank A.B. [Analytical chemistry in study and production of inorganic functional materials]. Kharkov, Institut monokristallov [Institute for Single Crystals], 2005, 305 p. (in Russian).
Golik V.M., Golik S.V., Trepachev S.A., Kuzmina N.V. [Determination of B, Si, P, S, Cl и Br in uranium materials by mass spectrometry with inductively coupled plasma]. Mass-spektrometriia [Mass spectrometry], 2010, vol. 7, no. 1, pp. 29-34 (in Russian).
Golik V.M., Trepachev S.A., Kisel T.A. [Determination of Th, Sm, Eu, Gd, Dy in uranium materials by mass spectrometry with inductively coupled plasma]. Sbornik VANT. Voprosy atomnoj nauki i tehniki. Tehnicheskaja fizika i avtomatizacija [Collected volume VANT. Problems of atomic science and technologies. Technical physics and automatic], 2006, vol. 60, pp. 123-129 (in Russian).
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